124 resultados para Milled powders


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Ti45Zr35Ni17Cu3 amorphous and icosahedral quasicrystal line (I-phase) powders were synthesized by mechanical alloying (MA) and subsequent annealing, the phase structure and hydrogen absorption properties of two powders were investigated. XRD analysis indicated that the MAed powder was an amorphous phase and annealed powder was an I-phase. Two alloy exhibited excellent hydrogen adsorption property and started to absorb hydrogen without induction time. PCT measurement showed that the plateau pressure of the amorphous powders was obviously higher than that of the I-phase powders. After the first hydrogen cycling, the partial amorphous phase changed to (Zr, Ti)H-2 phases, and the I-phase was steady. Similar hydride phases Ti2ZrH4 and (Zr, Ti)H-2 were also formed after the second hydrogen cycling for the amorphous and I-phase alloy powders.

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Icosahedral quasicrystalline Ti45Zr35Ni17Cu3 alloy was ball-milled with 30 mass% La0.9Zr0.1Ni4.5Al0.5 alloy (LaNi5 phase), the effect of the milling time on crystallographic and electrochemical characteristics of the alloy powder was investigated. The amount of amorphous phase increased with increasing milling time from 60 to 360 min, and the LaNi5 phase cannot be observed when milling time was 240 min or more. The maximum discharge capacity and high-rate dischargeability of milled alloy electrodes were obviously higher than those of the alloy electrode before milling. The cycling capacity retention rate after 40 cycles increased from 52.8% (t = 60 min) to 62.9% (t = 360 min).

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It is reported for the first time that horseradish peroxidase (HRP) immobilized on the active carbon can undergo a direct quasi-reversible electrochemical reaction. In addition, the immobilized HRP showed the stable bioelectrocatalytic activity for the reduction of H2O2.

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Ti45--xZr35--xNi17+2rCU3 (x=0, 2, 4, 6 and 8) icosahedral quasicrystalline phase (I-phase) alloy powders are synthesized by mechanical alloying and subsequent annealing techniques, and the crystallographic and electrochemical characteristics are investigated. The alloy powders are I-phase, and the quasi-lattice constant decreases with increasing x value. The maximum discharge capacity of the I-phase alloy electrodes first increases and then decreases with increasing x value, and the Ti39Zr26Ni29Cu3 I-phase electrode exhibits the highest discharge capacity of 274 mAh g(--1). The high-rate dischargeability at the discharge current density of 240mA g(--1) increases from 55.31 % (x= 0) to 74.24% (x= 8). Cycling stability also increases with increasing x value. The improvement in electrochemical characteristics may be ascribed to the added nickel, which not only improves the electrochemical activity, but also makes the alloy more resistant to oxidation.

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Ti45Zr35Ni17Cu3 amorphous and single icosahedral quasicrystalline powders were synthesized by mechanical alloying and subsequent annealing at 855 K. Microstructure and electrochemical properties of two alloy electrodes were characterized. When the temperature was enhanced from 303 to 343 K, the maximum discharge capacities increased from 86 to 329 mAh g(-1) and 76 to 312 mAh g(-1) for the amorphous and quasicrystalline alloy electrodes, respectively. Discharge capacities of two electrodes decrease distinctly with increasing cycle number. The I-phase is stable during charge/discharge cycles, and the main factors for its discharge capacity loss are the increase of the charge-transfer resistance and the pulverization of alloy particles. Besides the factors mentioned above, the formation of TiH2 and ZrH2 hydrides is another primary reason for the discharge capacity loss of the amorphous alloy electrode.

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A facile molten salt synthesis route was developed to prepare ZnTiO3 ceramic powders with simple oxides ZnO and TiO2 using sodium and potassium chloride eutectic salts as flux. The role of calcination temperature and time and the amount of salt addition to ZnTiO3 formation was investigated by thermogravimetry-differential thermal analysis, X-ray diffraction and Fourier transformation-infrared spectroscopy measurements. Pure hexagonal phase of ZnTiO3 could be obtained from the mixture of the simple oxides and the chlorides (50 mol% KCl, 20 times to oxides in molar ratio) heating at 800 degrees C for 6 h. The scanning electron microscopy images revealed the products were hexagonal sheets of about 1-3 mu m size. Increasing the amount of salt aids in reducing the crystal sizes of final ceramic powders because of diluting the solution.

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Icosahedral quasicrystalline Ti45Zr35Ni17Cu3 alloy powder was ball-milled with 20 mass% Ni, and the effect of the ball-milling time (t) on crystallographic and electrochemical characteristics were investigated. The amounts of icosahedral quasicrystalline and Ni phases decreased when ball-milling time increased from 30 to 180 min. The powder consisted of amorphous and (Ni and Ti) phases after 360 min of ball-milling. The maximum discharge capacity of the powder electrodes first increased from 89 (t = 0 min) to 192 mAh g(-1) (t = 180 min), and then decreased to 138 mAh g(-1) (t = 360 min). The high-rate dischargeability and the discharge capacity after 15 cycles increased with increasing ball-milling time.

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Stannic oxide xerogel was prepared by a forced hydrolysis method using SnCl4 as the precursor. The average grain sizes of the nanosized stannic oxide powders varied with the sintering temperatures. The powders were characterized by several different physico-chemical techniques. TEM was employed for the direct observation on grain sizes, shape and state of aggregation of the particles. XRD technique was used for the determination of the crystalline structure. Microstructural parameters of average crystallite size () and mean-square root microstrain (epsilon(2)>(1/2)) for the samples were calculated from the broadened values of the half-peak intensity of XRD. The atomic ratio between oxygen and tin in the surface region of the particles was estimated through the analysis of XPS. Attributing to lots of oxygen vacancies in the surface region of the nanoparticulates and the 'trapped electrons' in the vacancies, an ESR signal was observed in the sample sintered at 300 degrees C for 2 h. FTIR of the powders showed that intensity of the transverse optical mode of Sn-O stretching vibration increased with the sintering temperature while the bending vibration of O-Sn-O showed a blue shift. For Raman spectra, very important spectral characteristics such as variations of intensity and width of the bands were observed. A new Raman vibrational band located at 572 cm(-1) was identified in the samples of nanosized stannic oxide powders. Variation of these spectroscopic properties were strongly affected by grain size, shape and state of aggregation of the nanosized particulates.

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CeO2 nanometer powders of different sizes were prepared at low temperature by pyrolysis of amorphous citrate. XRD patterns show that CeO2 is cubic in structure, space group O-h(5)-F-M3M. TEM indicates that the prepared CeO2 is spherical in shape, and the particle size distribution is in narrow range. It was found that calcination temperature is a more important factor affecting the crystallite size of CeO2 than calcining time, the smaller the particle, the bigger the crystal lattice distortion, the worse the crystal growth. Solubility test of CeO2 in nitric acid reveals that the surface activity of CeO2 decreases with the increasing particle sizes. IR spectra analysis shows that the absorption of Ce-O bond is shifted to higher energy with the decrease of CeO2 particle sizes.

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A series of rare earth hydroxides and oxides ultrafine powders have been prepared by precipitation method using alcohol as dispersive and protective reagent. It was first to find that the crystallite size of cubic rare earth oxides had Lanthanide shrinking effect,but average crystal lattice distortion rate possessed lanthanide swelling effect;the change of diffraction intensity with atomic number presented an inverted W type, and double peaks structure was formed.

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The ultrafine LaFeO3 with particle size of 12 similar to 75nm was prepared by sol-gel method. In the process of gel to ultrafine powder, the weight loss reached 90%. The lowest forming temperature of single phase crystalline LaFeO3 ultrafine powder was ob